EP0545771B1 - Concurrent cyclone extractor - Google Patents
Concurrent cyclone extractor Download PDFInfo
- Publication number
- EP0545771B1 EP0545771B1 EP92403149A EP92403149A EP0545771B1 EP 0545771 B1 EP0545771 B1 EP 0545771B1 EP 92403149 A EP92403149 A EP 92403149A EP 92403149 A EP92403149 A EP 92403149A EP 0545771 B1 EP0545771 B1 EP 0545771B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- enclosure
- phase
- extractor according
- light
- dense phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000926 separation method Methods 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 30
- 238000000605 extraction Methods 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 23
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005243 fluidization Methods 0.000 claims description 4
- 230000006641 stabilisation Effects 0.000 claims description 4
- 238000011105 stabilization Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 2
- 239000008247 solid mixture Substances 0.000 claims description 2
- 238000009877 rendering Methods 0.000 claims 1
- 239000012071 phase Substances 0.000 description 103
- 239000003054 catalyst Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 15
- 229930195733 hydrocarbon Natural products 0.000 description 7
- 150000002430 hydrocarbons Chemical class 0.000 description 7
- 230000002093 peripheral effect Effects 0.000 description 7
- 239000004215 Carbon black (E152) Substances 0.000 description 6
- 235000021183 entrée Nutrition 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000003795 desorption Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000011044 inertial separation Methods 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04C—APPARATUS USING FREE VORTEX FLOW, e.g. CYCLONES
- B04C3/00—Apparatus in which the axial direction of the vortex flow following a screw-thread type line remains unchanged ; Devices in which one of the two discharge ducts returns centrally through the vortex chamber, a reverse-flow vortex being prevented by bulkheads in the central discharge duct
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04C—APPARATUS USING FREE VORTEX FLOW, e.g. CYCLONES
- B04C7/00—Apparatus not provided for in group B04C1/00, B04C3/00, or B04C5/00; Multiple arrangements not provided for in one of the groups B04C1/00, B04C3/00, or B04C5/00; Combinations of apparatus covered by two or more of the groups B04C1/00, B04C3/00, or B04C5/00
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/14—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts
- C10G11/18—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts according to the "fluidised-bed" technique
Definitions
- the invention relates to a cyclonic co-current extractor separator for separating solid particles from a gas.
- the feedstock is brought into contact with the catalyst in a reactor.
- the weight ratio of the catalyst flow rate to the feed rate is high and can generally vary from 1: 1 to 15: 1.
- the reaction products must be separated from the catalytic solids: the reaction is driven to secondary separation and the solids are recycled with, in some processes, regeneration of the catalyst.
- the present invention relates to equipment making it possible to rapidly separate the gaseous products and the catalyst, and to recover the products remaining on the catalyst after the separation.
- Certain catalytic conversion processes such as catalytic cracking of hydrocarbon feedstocks, require rapid separation of the gaseous products at the end of the catalytic reaction, to limit their thermal degradation.
- the catalyst is evacuated from the separation zone by a return leg which falls into the extractor.
- the products extracted from the catalyst are sent to the secondary separation stage, together with the products separated for separation, in a large volume enclosure where they are also highly exposed to the thermal degradation of the products.
- the present invention makes it possible to avoid these drawbacks by virtue of an advantageous use of the hydrodynamic properties of the gas / solid flow in a cyclonic (or cyclone) co-current separator, modified by adding a capacity, of large volume, in the solids outlet discharge enclosure.
- Figure 1 is shown a cyclonic extractor separator according to the invention.
- first external enclosure (1) of substantially regular elongated shape, having an axis (X) which is an axis of symmetry, having a substantially circular section of internal diameter D 1 and a length L 1 .
- Means can also be placed inside the inlet (4) to confer downstream, in the direction of circulation of the mixture M A , a helical or swirling movement, at least in the light phase L A of the mixture M A (figure 2).
- These means are usually inclined blades (see Figure 2).
- the tangential entry, the blades or other equivalent means constitute the means for introducing the mixture M A.
- the extractor separators according to the invention also comprise an inner enclosure (2) of elongated shape along an axis (X), of substantially circular section, arranged coaxially with respect to the enclosure (1), comprising at a distance ( Ls), less than (L 1 ), from the extreme level of the external input (4), an input (5) called internal input, of external diameter D 2 less than D 1 .
- the diameter of this internal inlet (5) is usually about 0.2 to about 0.9 times the diameter (D 1 ), most often about 0.4 to about 0.8 times the diameter (D 1 ) and preferably about 0.4 to 0.6 times the diameter (D 1 ).
- This distance (Ls) is usually about 0.2 to about 9.5 times the diameter (D 1 ) and most often about 0.5 to about 2 times the diameter (D 1 ).
- a relatively short distance of between 0.5 and 2 times the diameter (D 1 ) usually allows very rapid separation and good separation efficiency.
- the mixture separates at least in part into a dense phase D A and a light phase L A.
- the light phase L A penetrates, at least in part, into the inlet (5) and is evacuated towards the outside of the enclosure (1) by at least one conduit (6) which extends the enclosure (2).
- the extractor separators according to the invention also include an enclosure (3) called the second outer enclosure, of lower section, equal to or greater than that of the enclosure (1).
- the section of the enclosure (3) is at least equal to that of the enclosure (1) and most often it is greater than that of the enclosure (1). In general the section of the enclosure (3) is greater by at least 0.5% and most often by at least 25% than that of the enclosure (1).
- the enclosure (3) is connected to the enclosure (1) by an opening (7) of the same diameter D 1 as that of the enclosure (1).
- the enclosure (3) has an elongated shape along an axis and a substantially circular section of diameter D preferably greater than D1.
- the dense phase D A separated at least in part in zone A flows towards the enclosure (3), in the bottom of which it is collected, it then forms a bed (9) called fluidized.
- FIG. 2 also presents means (20) intended to evacuate the dense phase D A at least partially desorbed (that is to say that the reaction products retained by the solid have been at least partially extracted) constituted by an enclosure (21) independent of the enclosures (1), (2) and (3) forming a disengagement well.
- This enclosure has an inlet (22) into which the dense phase D A , collected in the enclosure (3), flows by gravity, and an outlet (23).
- the concentration in dense phase in the outlet (23) is maintained at the desired value thanks to the fluidization imposed in the enclosure (21) resulting from an injection of light phase L C by the means (24) and thanks to a line balancing (25) allowing the evacuation of the excess gas L C not entrained at the outlet (23) which will mix with phase L B.
- L C will be chosen for its desorbent properties.
- L C can be the same or different from L B.
- the light phase L C is used at least in part for the fluidization of the dense phase D A in the disengagement well.
- Figure 3 is a side view of an apparatus according to the invention, further comprising means for controlling the flow of the mixture M A in the tangential inlet (4).
- means for controlling the flow of the mixture M A in the tangential inlet (4) are usually desirable in the case of large flows of the various phases in the presence of using means allowing to favor the formation of the vortex, such as for example a helical roof descending (30) from the extreme level of the inlet.
- tangential or a volute for example internal (with planar winding) and allowing in addition to limit turbulence at the tangential inlet.
- the pitch of the propeller is about 0.01 to 3 times the value of L k and most often about 0.5 to about 1.5 times this value.
- a stabilization cone (31) fixed at the level of the inlet (4) along the axis opposite the inlet (5) for discharging the light phase L A.
- means (32) for breaking the flow to the wall of the solids are generally substantially planar blades whose plane includes the axis (X) of the enclosure (1). These means are preferably fixed on at least one wall of one of the enclosures (1) or (2). They are preferably fixed to the outer wall of the inner enclosure (2), preferably so that the distance L P between the internal inlet and the point of said blades closest to this internal inlet is approximately 0 to about 5 times the diameter D 1 and preferably from about 0.1 to about 1 time this diameter D 1 .
- the number of blades is usually at least 2 and for example from 2 to 50 and most often from 3 to 50. These blades usually have the characteristics of those described in patent application FR90 / 06937 in the name of the applicant.
- means aiming to improve the contacting between the light phase L B and the dense phase D A can be inserted in the fluidized bed (9) .
- These means are for example tubes (107) arranged in regular rows on the section of the enclosure (3), and shown in Figure (5).
- tubes of diameter varying between 0.02 and 0.08 m arranged at intervals of at least once the diameter of the tubes.
- These tubes could advantageously be used to heat the fluidized bed and promote the desorption of the reaction products.
- the residence time of the solids constituting the dense phase D A in the fluidized bed (9) is usually from about 10 (s) seconds to about 15 (min) minutes. Most often this residence time is from about 30 s to about 10 min.
- the extractor separators according to the invention can be used for the rapid separation, from a mixture M A , comprising a dense phase D A and a light phase L A , of said dense phase and of said light phase and extraction of the products adsorbed by said dense phase D A.
- the mixture to be separated can be a mixture obtained at the end of a chemical reaction and comprising at least one phase which contributes to this reaction.
- the volume flow rate Q 2 of mixture M A gas / incoming catalyst is 8.3 X 10 -3 m 3 / s which corresponds to a surface speed of 25 m / s for the light phase present in the mixture M A to l entry of the extractor separator.
- the flow rate of the light phase L B of extradion (in volume Q 1 ) having varied from 0 to 15% of the flow rate Q 2 . Under these conditions, the speed of passage through the peripheral space (11) is less than 20 cm / s.
- the device which is the subject of the present invention has major advantages over the various devices which are proposed in the literature. It allows rapid separation, diluted phase extraction and deep dense phase extraction.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Cyclones (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Separating Particles In Gases By Inertia (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Description
L'invention concerne un séparateur extracteur cyclonique à co-courant pour séparer les particules solides d'un gaz.The invention relates to a cyclonic co-current extractor separator for separating solid particles from a gas.
Dans l'industrie pétrolière, et plus précisément dans les procédés de conversion de charge hydrocarbonée sur catalyseur effectués en lit circulant, la charge est mise au contact du catalyseur dans un réacteur. Le rapport en poids du débit du catalyseur sur le débit de charge est élevé et peut varier en général de 1 : 1 à 15 : 1. A la sortie du réacteur, il faut séparer les produits de la réaction des solides catalytiques : les produits de la réaction sont entraînés vers une séparation secondaire et les solides sont recyclés avec, dans certains procédés, la régénération du catalyseur.In the petroleum industry, and more precisely in the conversion process of hydrocarbon feedstock to catalyst carried out in a circulating bed, the feedstock is brought into contact with the catalyst in a reactor. The weight ratio of the catalyst flow rate to the feed rate is high and can generally vary from 1: 1 to 15: 1. At the outlet of the reactor, the reaction products must be separated from the catalytic solids: the reaction is driven to secondary separation and the solids are recycled with, in some processes, regeneration of the catalyst.
Avant de recycler le catalyseur, il est important de désorber les produits hydrocarbonés encore présents à la surface ou à l'intérieur du catalyseur pour récupérer les produits de la réaction qui seraient perdus sans cela.Before recycling the catalyst, it is important to desorb the hydrocarbon products still present on the surface or inside the catalyst to recover the reaction products which would otherwise be lost.
La présente invention concerne un équipement permettant d'effectuer une séparation rapide des produits gazeux et du catalyseur, et de récupérer les produits restant sur le catalyseur à l'issue de la séparation.The present invention relates to equipment making it possible to rapidly separate the gaseous products and the catalyst, and to recover the products remaining on the catalyst after the separation.
Certains procédés de conversion catalytique, tels que le craquage catalytique de charges hydrocarbonées, nécessitent une séparation rapide des produits gazeux à la fin de la réaction catalytique, pour limiter leur dégradation thermique.Certain catalytic conversion processes, such as catalytic cracking of hydrocarbon feedstocks, require rapid separation of the gaseous products at the end of the catalytic reaction, to limit their thermal degradation.
Il peut alors être avantageux d'utiliser des cyclones connectés directement au réacteur (par exemple au sommet d'un réacteur à lit ascendant) plutôt que de se contenter d'une séparation inertielle dans un gros volume qui est synonyme de long temps de séjour. Des exemples de procédés de conversion de coupes hydrocarbonées avec séparation rapide sont donnés par exemple dans le brevet de Rod et al. (US4946656) où la séparation est effectuée dans un cyclone dit "à rebours" ou dans le brevet de Gauthier et al. (demande de brevet FR90/06937 non publiée au jour du dépôt de la présente demande) où la séparation est effectuée dans un cyclone à co-courant.It may then be advantageous to use cyclones connected directly to the reactor (for example at the top of a rising bed reactor) rather than being satisfied with an inertial separation in a large volume which is synonymous with long residence time. Examples of processes for converting hydrocarbon cuts with rapid separation are given, for example, in the patent of Rod et al. (US4946656) where the separation is carried out in a cyclone called "reverse" or in the patent of Gauthier et al. (patent application FR90 / 06937 not published on the date of filing of this application) where the separation is carried out in a co-current cyclone.
La séparation rapide des effluents de craquage catalytique de coupes hydrocarbonées permet généralement de gagner en sélectivité, en évitant de former les produits tels que le fuel gaz ou le coke qui sont faiblement valorisés en très grandes quantités, et en privilégiant plutôt la sélectivité en essence et en coupe d'huile légère (LCO) (en anglais Light Cycle Oil) dont la valorisation est nettement supérieure. Cependant, si cette séparation rapide n'est pas accompagnée d'une extraction (stripage) efficace, et placée à proximité, dans le temps, de la phase de séparation, on perdra une partie des avantages de la séparation rapide, en gardant adsorbés sur le catalyseur des produits valorisables qui seront dégradés thermiquement. De même, les produits désorbés du catalyseur doivent être évacués rapidement de l'enceinte dans laquelle est effectuée l'extraction. Par exemple, dans le brevet US4946656, le catalyseur est évacué de la zone de séparation par une jambe de retour qui tombe dans l'extracteur. Les produits extraits du catalyseur sont envoyés vers l'étape de séparation secondaire, en commun avec les produits séparés à la séparation, dans une enceinte de grand volume où ils sont eux aussi fortement exposés à la dégradation thermique des produits.The rapid separation of catalytic cracking effluents from hydrocarbon cuts generally makes it possible to gain in selectivity, by avoiding the formation of products such as fuel gas or coke which are poorly valued in very large quantities, and by favoring rather the selectivity in gasoline and in light oil cut (LCO) (in English Light Cycle Oil) whose recovery is clearly higher. However, if this rapid separation is not accompanied by an effective extraction (stripping), and placed close, in time, to the separation phase, we will lose part of the advantages of rapid separation, by keeping adsorbed on the catalyst for recoverable products which will be thermally degraded. Likewise, the products desorbed from the catalyst must be removed quickly from the enclosure in which the extraction is carried out. For example, in patent US4946656, the catalyst is evacuated from the separation zone by a return leg which falls into the extractor. The products extracted from the catalyst are sent to the secondary separation stage, together with the products separated for separation, in a large volume enclosure where they are also highly exposed to the thermal degradation of the products.
Il est également possible comme dans le brevet français 83/20435 d'inclure une zone d'extraction dense à la base d'un cyclone à rebours, intercalée par exemple entre la zone de retournement du vortex et la sortie des solides. Cette configuration présente l'avantage de séparer les produits adsorbés sur le catalyseur grâce à un courant gazeux injecté dans la même enceinte de séparation primaire gaz-particules de catalyseur. Les produits gazeux de la réaction sont alors prélevés dans la partie supérieure de l'enceinte effectuant la séparation. L'inconvénient d'un tel appareil est qu'il faut, afin de garder des performances de séparation acceptables, placer un déflecteur entre la zone d'extraction et la zone de séparation. Ce déflecteur permet de guider le vortex gazeux lors de son retoumement dans l'enceinte de séparation. Il est nécessaire de fixer cet élément matériellement au corps de l'enceinte de séparation. Les fixations vont nuire à l'écoulement régulier des solides aux parois et, exposées à des écoulements continus de solides, elles risquent de s'éroder rapidement, ce qui pourrait entraîner un dysfonctionnement de l'appareil.It is also possible as in French patent 83/20435 to include a dense extraction zone at the base of a reverse cyclone, interposed for example between the vortex reversal zone and the solids outlet. This configuration has the advantage of separating the products adsorbed on the catalyst by means of a gas stream injected into the same primary separation chamber for gas-catalyst particles. The gaseous products of the reaction are then taken from the upper part of the enclosure carrying out the separation. The disadvantage of such an apparatus is that, in order to keep acceptable separation performance, place a deflector between the extraction zone and the separation zone. This deflector guides the gas vortex when it returns to the separation enclosure. It is necessary to fix this element materially to the body of the separation enclosure. The fasteners will interfere with the regular flow of solids to the walls and, exposed to continuous flows of solids, they may erode quickly, which could cause the device to malfunction.
La présente invention permet d'éviter ces inconvénients grâce à une utilisation avantageuse des propriétés hydrodynamiques de l'écoulement gaz/solide dans un séparateur cyclonique (ou cyclone) à co-courant, modifié par adjonction d'une capacité, de volume important, dans l'enceinte d'évacuation de la sortie des solides.The present invention makes it possible to avoid these drawbacks by virtue of an advantageous use of the hydrodynamic properties of the gas / solid flow in a cyclonic (or cyclone) co-current separator, modified by adding a capacity, of large volume, in the solids outlet discharge enclosure.
Plus précisément, l'invention concerne un séparateur extracteur, cyclonique à co-courant, pour la séparation d'un mélange gaz/solide M A, comprenant au moins une base dense D A et une phase légère L A, en au moins une phase dense et en au moins une phase légère, avec extraction des gaz sorbés par le solide, ledit séparateur extracteur comprenant:
- une enceinte (1) dite première enceinte extérieure, de forme allongée le long d'un axe (X), de section sensiblement circulaire de diamètre interne D1, de longueur L1, comprenant à une première extrémité, des moyens pour l'introduction du mélange M A par une entrée (4) dite externe, lesdits moyens permettant de conférer, au moins à la phase légère L A, un mouvement hélicoïdal dans la direction de l'écoulement du mélange M A dans ladite enceinte,
- une enceinte (2) dite intérieure, de forme allongée le long de l'axe (X), de section sensiblement circulaire de diamètre D2 inférieur à D1, de longueur L2 inférieure à L1, dont l'extrémité proche de l'entrée (4) externe située à une distance Ls inférieure à L1 du niveau extrême de l'entrée (4) externe constitue l'entrée (5) dite interne par laquelle pénètre au moins une partie de la phase légère L A, ladite enceinte étant prolongée par au moins un conduit (6) permettant l'évacuation de la phase légère L A séparée à l'extérieur de la première enceinte extérieure,
- une enceinte (3) dite seconde enceinte extérieure, présentant un axe de symétrie sensiblement vertical, raccordée à ladite première enceinte par une ouverture de diamètre D1, ladite seconde enceinte recueillant la phase dense D A séparée comporte des moyens (10) pour l'injection d'une phase légère d'extraction L B, l'injection ayant lieu à contre-courant de l'écoulement de la phase dense séparée et au moins en partie dans ladite phase dense qui est fluidisée au moins en partie, et comporte au moins une sortie (12) pour la récupération de la phase dense D A désorbée au moins en partie. Cette phase légère dite L B est évacuée du séparateur extracteur en mélange avec la phase L A par l'enceinte (2) et le conduit (6).
- an enclosure (1) called the first external enclosure, of elongated shape along an axis (X), of substantially circular section of internal diameter D 1 , of length L 1 , comprising at a first end, means for the introduction of the mixture M A by a so-called external inlet (4), said means making it possible to confer, at least on the light phase L A , a helical movement in the direction of the flow of the mixture M A in said enclosure,
- an enclosure (2) called interior, of elongated shape along the axis (X), of substantially circular section of diameter D 2 less than D 1 , of length L 2 less than L 1 , the end of which is close to l external input (4) located at a distance Ls less than L 1 from the extreme level of the external input (4) constitutes the internal input (5) through which at least part of the light phase L A penetrates, said enclosure being extended by at least one conduit (6) allowing the evacuation of the light phase L A separated outside the first external enclosure,
- an enclosure (3) called the second external enclosure, having a substantially vertical axis of symmetry, connected to said first enclosure by an opening of diameter D1, said second enclosure collecting the dense dense phase D A comprises means (10) for injection a light extraction phase L B , the injection taking place against the flow of the separated dense phase and at least in part in said dense phase which is fluidized at least in part, and comprises at least an outlet (12) for recovering the dense phase D A desorbed at least in part. This light phase called L B is removed from the extractor separator in mixture with phase L A through the enclosure (2) and the conduit (6).
Pour faciliter la compréhension, l'invention sera décrite à partir des figures, sans pour autant limiter sa portée auxdites figures.To facilitate understanding, the invention will be described from the figures, without however limiting its scope to said figures.
Chacune des figures 1 à 5 représente un mode de réalisation de l'invention.Each of Figures 1 to 5 shows an embodiment of the invention.
Sur la figure 1 est représenté un séparateur extracteur cyclonique selon l'invention.In Figure 1 is shown a cyclonic extractor separator according to the invention.
Il comporte une première enceinte extérieure (1), de forme allongée sensiblement régulière, ayant un axe (X) qui est un axe de symétrie, ayant une section sensiblement circulaire de diamètre interne D1 et une longueur L1.It comprises a first external enclosure (1), of substantially regular elongated shape, having an axis (X) which is an axis of symmetry, having a substantially circular section of internal diameter D 1 and a length L 1 .
L'axe (X) est en général sensiblement vertical (figures 1 à 4) mais il peut être sensiblement horizontal (figure 5).The axis (X) is generally substantially vertical (Figures 1 to 4) but it can be substantially horizontal (Figure 5).
A l'une de ses extrémités, l'enceinte (1) comporte une entrée (4) dite externe par laquelle le mélange M A à traiter arrive. De préférence, le mélange M A est introduit par une entrée (4) tangentielle suivant une direction sensiblement perpendiculaire à l'axe de l'enceinte extérieure. Cette entrée tangentielle a de préférence une section rectangulaire ou carrée dont le côté parallèle à l'axe de l'enceinte extérieure a une dimension (Lk) habituellement d'environ 0,25 à environ 1 fois le diamètre D1, et le côté perpendiculaire à l'axe de l'enceinte extérieure a une dimension (hk) habituellement d'environ 0,05 à environ 0,5 fois le diamètre D1.At one of its ends, the enclosure (1) has an said external inlet (4) through which the mixture M A to be treated arrives. Preferably, the mixture M A is introduced by a tangential inlet (4) in a direction substantially perpendicular to the axis of the outer enclosure. This tangential entry preferably has a rectangular or square section whose side parallel to the axis of the outer enclosure has a dimension (Lk) usually from about 0.25 to about 1 times the diameter D 1 , and the perpendicular side at the axis of the outer enclosure has a dimension (hk) usually from about 0.05 to about 0.5 times the diameter D 1 .
Des moyens peuvent également être placés à l'intérieur de l'entrée (4) pour conférer en aval, dans le sens de circulation du mélange M A, un mouvement hélicoïdal ou tourbillonnant, au moins à la phase légère L A du mélange M A (figure 2). Ces moyens sont habituellement des pales inclinées (voir figure 2). L'entrée tangentielle, les pales ou autres moyens équivalents constituent les moyens d'introduction du mélange M A.Means can also be placed inside the inlet (4) to confer downstream, in the direction of circulation of the mixture M A , a helical or swirling movement, at least in the light phase L A of the mixture M A (figure 2). These means are usually inclined blades (see Figure 2). The tangential entry, the blades or other equivalent means constitute the means for introducing the mixture M A.
Les séparateurs extracteurs selon l'invention comportent également une enceinte intérieure (2) de forme allongée le long d'un axe (X), de section sensiblement circulaire, disposée coaxialement par rapport à l'enceinte (1), comprenant à une distance (Ls), inférieure à (L1), du niveau extrême de l'entrée externe (4), une entrée (5) dite entrée interne, de diamètre externe D2 inférieur à D1. Le diamètre de cette entrée interne (5) est habituellement d'environ 0,2 à environ 0,9 fois le diamètre (D1), le plus souvent d'environ 0,4 à environ 0,8 fois le diamètre (D1) et de préférence d'environ 0,4 à 0,6 fois le diamètre (D1). Cette distance (Ls) est habituellement d'environ 0,2 à environ 9,5 fois le diamètre (D1) et le plus souvent d'environ 0,5 à environ 2 fois le diamètre (D1). Une distance relativement courte comprise entre 0,5 et 2 fois le diamètre (D1) permet habituellement une séparation très rapide et une bonne efficacité de séparation.The extractor separators according to the invention also comprise an inner enclosure (2) of elongated shape along an axis (X), of substantially circular section, arranged coaxially with respect to the enclosure (1), comprising at a distance ( Ls), less than (L 1 ), from the extreme level of the external input (4), an input (5) called internal input, of external diameter D 2 less than D 1 . The diameter of this internal inlet (5) is usually about 0.2 to about 0.9 times the diameter (D 1 ), most often about 0.4 to about 0.8 times the diameter (D 1 ) and preferably about 0.4 to 0.6 times the diameter (D 1 ). This distance (Ls) is usually about 0.2 to about 9.5 times the diameter (D 1 ) and most often about 0.5 to about 2 times the diameter (D 1 ). A relatively short distance of between 0.5 and 2 times the diameter (D 1 ) usually allows very rapid separation and good separation efficiency.
Sous l'effet du vortex créé, le mélange se sépare au moins en partie en une phase dense D A et une phase légère L A. La phase légère L A pénètre, au moins en partie, dans l'entrée (5) et est évacuée vers l'extérieur de l'enceinte (1) par au moins un conduit (6) qui prolonge l'enceinte (2).Under the effect of the vortex created, the mixture separates at least in part into a dense phase D A and a light phase L A. The light phase L A penetrates, at least in part, into the inlet (5) and is evacuated towards the outside of the enclosure (1) by at least one conduit (6) which extends the enclosure (2).
Une zone (A) de séparation est ainsi définie entre le niveau extrême de l'entrée (4) et approximativement le niveau de l'entrée (5).A separation zone (A) is thus defined between the extreme level of the entry (4) and approximately the level of the entry (5).
Les séparateurs extracteurs selon l'invention comportent également une enceinte (3) dite seconde enceinte extérieure, de section inférieure, égale ou supérieure à celle de l'enceinte (1). De préférence la section de l'enceinte (3) est au moins égale à celle de l'enceinte (1) et le plus souvent elle est supérieure à celle de l'enceinte (1). En général la section de l'enceinte (3) est supérieure d'au moins 0,5 % et le plus souvent d'au moins 25 % à celle de l'enceinte (1). L'enceinte (3) est raccordée à l'enceinte (1) par une ouverture (7) de même diamètre D1 que celui de l'enceinte (1).The extractor separators according to the invention also include an enclosure (3) called the second outer enclosure, of lower section, equal to or greater than that of the enclosure (1). Preferably the section of the enclosure (3) is at least equal to that of the enclosure (1) and most often it is greater than that of the enclosure (1). In general the section of the enclosure (3) is greater by at least 0.5% and most often by at least 25% than that of the enclosure (1). The enclosure (3) is connected to the enclosure (1) by an opening (7) of the same diameter D 1 as that of the enclosure (1).
De préférence, l'enceinte (3) a une forme allongée le long d'un axe et une section sensiblement circulaire de diamètre D de préférence supérieur à D1.Preferably, the enclosure (3) has an elongated shape along an axis and a substantially circular section of diameter D preferably greater than D1.
Avantageusement, l'enceinte (3) est dans le prolongement de l'axe (X) de l'enceinte (1). La figure 1 le montre, avec une surface (8) conique de raccordement.Advantageously, the enclosure (3) is in the extension of the axis (X) of the enclosure (1). Figure 1 shows, with a conical connection surface (8).
La phase dense D A séparée au moins en partie dans la zone A s'écoule vers l'enceinte (3), dans le fond de laquelle elle est recueillie, elle forme alors un lit (9) dit fluidisé.The dense phase D A separated at least in part in zone A flows towards the enclosure (3), in the bottom of which it is collected, it then forms a bed (9) called fluidized.
L'enceinte (3) comporte des moyens (10) pour l'injection dans la phase D A d'une phase légère L B d'extraction, à contre-courant de l'écoulement de la phase dense D A séparée.The enclosure (3) comprises means (10) for the injection into phase D A of a light phase L B of extraction, against the flow of the flow of the dense phase D A separated.
En effet, naturellement dans un cyclone à co-courant, la phase légère a tendance à circuler en partie dans l'espace périphérique (11) situé entre l'enceinte extérieure (1) et l'enceinte intérieure (2) avant de sortir du séparateur extracteur grâce à cette enceinte (2).Indeed, naturally in a co-current cyclone, the light phase tends to circulate partly in the peripheral space (11) located between the outer enclosure (1) and the inner enclosure (2) before leaving the separator extractor thanks to this enclosure (2).
La conséquence est que dans ledit espace périphérique, les solides restent maintenus à la paroi sous l'effet de la force centrifuge bien au-delà du niveau où est prélevée la phase légère. En contrepartie, un rétromélange qui peut être important dans certains cas peut apparaître dans ledit espace périphérique.The consequence is that in said peripheral space, the solids remain held at the wall under the effect of centrifugal force well beyond the level where the phase is taken slight. In return, a back-mixing which may be significant in certain cases may appear in said peripheral space.
Un moyen simple visant à réduire la circulation de la phase légère L A dans cet espace est d'injecter en petites quantités une phase légère L B à contre-courant de la phase légère L A. L'injection de la phase légère L B peut s'effectuer en divers endroits simultanément. Par ailleurs, il est également possible d'injecter dans ce dernier cas des phases légères de compositions différentes. Si l'injection de la phase légère L B est convenablement dosée, les solides restent en majorité maintenus en périphérie au niveau de l'entrée (5) de l'enceinte (2) de prélèvement des phases légères, ce qui permet d'éviter que les solides soient entraînés vers l'enceinte d'évacuation des phases légères en quantités trop importantes. Simultanément, la phase légère L A est repoussée par la phase légère L B injectée à contre-courant ce qui limite le rétromélange.A simple way to reduce the circulation of the light phase L A in this space is to inject in small quantities a light phase L B against the current of the light phase L A. The injection of the light phase L B can be carried out in various places simultaneously. Furthermore, it is also possible to inject in the latter case light phases of different compositions. If the injection of the light phase L B is properly dosed, the majority of the solids are kept at the periphery at the inlet (5) of the enclosure (2) for sampling the light phases, which makes it possible to avoid that the solids are entrained towards the evacuation enclosure of the light phases in too large quantities. Simultaneously, the light phase L A is repelled by the light phase L B injected against the current, which limits the back-mixing.
Il y a avantage à utiliser ces propriétés hydrodynamiques pour limiter le rétromélange de la phase légère gazeuse L A séparée comme il vient d'être mentionné, mais également pour favoriser la bonne extraction des produits. En effet, les vapeurs de la phase légère L B injectées à contre-courant qui circulent dans l'espace périphérique (11) permettent d'effectuer une extraction très rapide des produits de réaction encore présents sur le catalyseur.It is advantageous to use these hydrodynamic properties to limit the backmixing of the separated light gas phase L A as just mentioned, but also to promote good extraction of the products. In fact, the vapors of the light phase L B injected against the current which circulate in the peripheral space (11) make it possible to carry out a very rapid extraction of the reaction products still present on the catalyst.
Par ailleurs, ladite injection confère dans l'enceinte (3) à la phase dense D A les propriétés d'un milieu dit fluidisé. Le taux de vide du lit est compris entre 35 et 75 % de préférence.Furthermore, said injection confers in the enclosure (3) the dense phase D A the properties of a so-called fluidized medium. The vacuum level of the bed is preferably between 35 and 75%.
La phase légère LB est injectée sous forme gazeuse. Elle comprend par exemple de la vapeur d'eau, de l'azote, une charge hydrocarbonée vaporisée à bas point d'ébullition.The light phase L B is injected in gaseous form. It includes for example steam, nitrogen, a vaporized hydrocarbon feed with low boiling point.
Les moyens d'injection (10) sont situés dans le fond de l'enceinte (3) pour l'injection dans la phase dense D A. Ce sont par exemple des orifices agencés régulièrement dans une couronne centrée sur l'axe de l'enceinte (3). On définit ainsi, à partir de la zone A de séparation, une zone B dans laquelle la phase dense D A subit un écoulement descendant et où, au moins une partie de la phase L A s'écoule en maintenant la phase dense D A à la paroi, la phase légère L A est évacuée, une zone C dans laquelle la phase dense D A continue son écoulement descendant et subit une désorption partielle et enfin une zone D dans laquelle la phase dense maintenue en lit fluidisé, est partiellement désorbée et est partiellement évacuée.The injection means (10) are located in the bottom of the enclosure (3) for injection into the dense phase D A. These are for example orifices regularly arranged in a crown centered on the axis of the enclosure (3). We thus define, from the separation zone A, a zone B in which the dense phase D A undergoes a downward flow and where, at least part of the phase L A flows while maintaining the dense phase D A at the wall, the light phase L A is evacuated, a zone C in which the dense phase D A continues its downward flow and undergoes partial desorption and finally a zone D in which the dense phase maintained in a fluidized bed, is partially desorbed and is partially removed.
Les moyens (12) pour l'évacuation d'une partie au moins de la phase dense D A sont disposés dans la partie inférieure de l'enceinte (3), latéralement (puits de désengagement par exemple sur la figure 2) ou axialement (puits cylindrique vertical par exemple sur la figure 1).The means (12) for evacuating at least part of the dense phase D A are arranged in the lower part of the enclosure (3), laterally (disengagement well for example in FIG. 2) or axially ( vertical cylindrical well for example in Figure 1).
La figure 2 représente un autre mode de réalisation du séparateur extracteur selon l'invention, qui diffère de celui représenté sur la figure 1, par les moyens mis en oeuvre pour conférer à la phase dense D A et la phase légère L A la vorticité nécessaire à la séparation des phases. Sur la figure 1, les moyens représentés sont une entrée dite tangentielle constituée par un conduit sensiblement horizontal, arrivant tangentiellement à l'enceinte (1). Sur la figure 2, les moyens d'introduction mis en oeuvre pour conférer à la phase dense D A et à la phase légère L A la vorticité nécessaire, à la séparation des phases dans la zone A, sont constitués de pales ou hélices (26) placées axialement dans l'entrée (4), également coaxiale à l'enceinte (1). L'appareil décrit sur la figure 2 se différencie de celui décrit sur la figure (1) également par le nombre de conduits (6) prolongeant l'enceinte (2) pour évacuer la phase légère L A. En effet, afin de diminuer la taille des appareils supplémentaires aptes à récupérer les particules qui n'auraient pas été séparées dans l'appareil de l'invention, il peut être avantageux de diviser le flux de phase légère L A en plusieurs flux, par exemple au moyen de plusieurs conduits (6) comme montré sur la figure 2. Ce(s) conduit(s) est soit disposé de manière à ce que la phase légère soit évacuée dans une direction sensiblement axiale par rapport à l'enceinte (1) (voir par exemple figure 5), soit dans une direction sensiblement perpendiculaire à l'axe de l'enceinte (1) (voir par exemple les figures 1 à 4).FIG. 2 represents another embodiment of the extractor separator according to the invention, which differs from that shown in FIG. 1, by the means used to give the dense phase D A and the light phase L A the necessary vorticity at the separation of the phases. In FIG. 1, the means shown are a so-called tangential inlet constituted by a substantially horizontal conduit, arriving tangentially to the enclosure (1). In FIG. 2, the introduction means used to give the dense phase D A and the light phase L A the necessary vorticity, for the separation of the phases in zone A, consist of blades or propellers (26 ) placed axially in the inlet (4), also coaxial with the enclosure (1). The device described in Figure 2 differs from that described in Figure (1) also by the number of conduits (6) extending the enclosure (2) to evacuate the light phase L A. In fact, in order to reduce the size of the additional devices capable of recovering the particles which would not have been separated in the device of the invention, it may be advantageous to divide the stream of light phase L A into several streams, by example by means of several conduits (6) as shown in Figure 2. This (s) conduit (s) is either arranged so that the light phase is discharged in a substantially axial direction relative to the enclosure (1 ) (see for example Figure 5), or in a direction substantially perpendicular to the axis of the enclosure (1) (see for example Figures 1 to 4).
La figure 2 présente également des moyens (20) destinés à évacuer la phase dense D A au moins en partie désorbée (c'est-à-dire que les produits de réaction retenus par le solide ont été au moins en partie extraits) constitués par une enceinte (21) indépendante des enceintes (1), (2) et (3) formant un puits de désengagement. Cette enceinte possède une entrée (22) dans laquelle la phase dense D A, recueillie dans l'enceinte (3), s'écoule par gravité, et une sortie (23). La concentration en phase dense dans la sortie (23) est maintenue à la valeur désirée grâce à la fluidisation imposée dans l'enceinte (21) résultant d'une injection de phase légère L C par les moyens (24) et grâce à une ligne d'équilibrage (25) permettant d'évacuer l'excès de gaz L C non entraîné à la sortie (23) qui se mélangera avec la phase L B. Avantageusement L C sera choisi pour ses propriétés désorbantes. L C peut être identique ou différent de L B. La phase légère L C sert au moins en partie à la fluidisation de la phase dense D A dans le puits de désengagement.FIG. 2 also presents means (20) intended to evacuate the dense phase D A at least partially desorbed (that is to say that the reaction products retained by the solid have been at least partially extracted) constituted by an enclosure (21) independent of the enclosures (1), (2) and (3) forming a disengagement well. This enclosure has an inlet (22) into which the dense phase D A , collected in the enclosure (3), flows by gravity, and an outlet (23). The concentration in dense phase in the outlet (23) is maintained at the desired value thanks to the fluidization imposed in the enclosure (21) resulting from an injection of light phase L C by the means (24) and thanks to a line balancing (25) allowing the evacuation of the excess gas L C not entrained at the outlet (23) which will mix with phase L B. Advantageously L C will be chosen for its desorbent properties. L C can be the same or different from L B. The light phase L C is used at least in part for the fluidization of the dense phase D A in the disengagement well.
La figure 3 est une vue de côté d'un appareil selon l'invention, comportant en outre des moyens pour contrôler l'écoulement du mélange M A dans l'entrée tangentielle (4). En effet, il est habituellement souhaitable dans le cas de débits importants des diverses phases en présence d'utiliser des moyens permettant de favoriser la formation du vortex, comme par exemple un toit hélicoïdal descendant (30) à partir du niveau extrême de l'entrée tangentielle ou une volute par exemple interne (à enroulement plan) et permettant en plus de limiter la turbulence au niveau de l'entrée tangentielle. Habituellement, dans le cas d'un toit hélicoïdal descendant, le pas de l'hélice est d'environ 0,01 à 3 fois la valeur de Lk et le plus souvent d'environ 0,5 à environ 1,5 fois cette valeur. Pour stabiliser le vortex dans sa progression, on peut également prévoir un cône de stabilisation (31) fixé au niveau de l'entrée (4) selon l'axe en vis-à-vis de l'entrée (5) d'évacuation de la phase légère L A. Sur la figure (3) sont également représentés des moyens (32) pour briser l'écoulement à la paroi des solides. Ces moyens (32) sont généralement des pales sensiblement planes dont le plan comporte l'axe (X) de l'enceinte (1). Ces moyens sont de préférence fixés sur au moins une paroi de l'une des enceintes (1) ou (2). Ils sont de préférence fixés à la paroi extérieure de l'enceinte intérieure (2), de préférence de sorte que la distance LP entre l'entrée interne et le point desdites pales le plus proche de cette entrée interne soit d'environ 0 à environ 5 fois le diamètre D1 et de préférence d'environ 0,1 à environ 1 fois ce diamètre D1. Le nombre de pales est habituellement d'au moins 2 et par exemple de 2 à 50 et le plus souvent de 3 à 50. Ces pales ont habituellement les caractéristiques de celles décrites dans la demande de brevet FR90/06937 au nom de la demanderesse.Figure 3 is a side view of an apparatus according to the invention, further comprising means for controlling the flow of the mixture M A in the tangential inlet (4). Indeed, it is usually desirable in the case of large flows of the various phases in the presence of using means allowing to favor the formation of the vortex, such as for example a helical roof descending (30) from the extreme level of the inlet. tangential or a volute, for example internal (with planar winding) and allowing in addition to limit turbulence at the tangential inlet. Usually, in the case of a descending helical roof, the pitch of the propeller is about 0.01 to 3 times the value of L k and most often about 0.5 to about 1.5 times this value. To stabilize the vortex in its progression, it is also possible to provide a stabilization cone (31) fixed at the level of the inlet (4) along the axis opposite the inlet (5) for discharging the light phase L A. Also shown in Figure (3) are means (32) for breaking the flow to the wall of the solids. These means (32) are generally substantially planar blades whose plane includes the axis (X) of the enclosure (1). These means are preferably fixed on at least one wall of one of the enclosures (1) or (2). They are preferably fixed to the outer wall of the inner enclosure (2), preferably so that the distance L P between the internal inlet and the point of said blades closest to this internal inlet is approximately 0 to about 5 times the diameter D 1 and preferably from about 0.1 to about 1 time this diameter D 1 . The number of blades is usually at least 2 and for example from 2 to 50 and most often from 3 to 50. These blades usually have the characteristics of those described in patent application FR90 / 06937 in the name of the applicant.
L'avantage d'utiliser de tels moyens est de briser l'écoulement à la paroi des solides. Ils permettent également d'uniformiser la répartition de la phase dense D A arrivant dans l'enceinte (3), ce qui est très favorable à l'extraction des produits sorbés. Enfin, ils permettent de répartir de façon homogène les solides coulant à la paroi sur toute la section périphérique de l'enceinte (1) entourant l'enceinte (2) ou le(s) conduit(s) (6). Il faut noter que, contrairement à l'application en séparation rapide (demande de brevet FR90/06937 non encore publiée), le rôle des moyens (32) n'est pas seulement de limiter la progression du vortex et de diminuer le rétromélange, car ici l'injection de la phase légère dextraction L B assure en partie cette fonction. Ces moyens (32) pourraient également être des déflecteurs visant à améliorer le contact entre la phase descendante D A et la phase légère d'extraction L B.The advantage of using such means is to break the flow to the wall of the solids. They also make it possible to standardize the distribution of the dense phase D A arriving in the enclosure (3), which is very favorable for the extraction of the sorbed products. Finally, they allow the solids flowing to the wall to be distributed homogeneously over the entire peripheral section of the enclosure (1) surrounding the enclosure (2) or the conduit (s) (6). It should be noted that, unlike the rapid separation application (patent application FR90 / 06937 not yet published), the role of the means (32) is not only to limit the progression of the vortex and to reduce the back-mixing, because here the injection of the light extraction phase L B partially performs this function. These means (32) could also be deflectors aimed at improving the contact between the descending phase D A and the light extraction phase L B.
Sur la figure 4, des moyens (40) ont été rajoutés, permettant l'introduction de phase légère d'extraction LB au-dessus du lit de la phase dense D A, la phase légère L B étant injectée à contre-courant de la phase dense D A qui s'écoule de la zone de séparation A vers l'enceinte (3). Cette injection permet de diminuer dans la phase diluée de solides (circulant de la zone A vers l'enceinte (3)) la pression partielle de gaz désorbés (hydrocarbures par exemple) remontant de la zone d'extraction D vers l'enceinte (2) d'évacuation, et donc de favoriser la désorption.
Les moyens (40) sont des moyens classiques d'introduction de gaz (tels qu'une tuyauterie droite ou circulaire munie d'orifices) devant respecter une distribution de fluide aussi homogène que possible. Ces moyens (40) sont donc disposés au niveau de la zone C, c'est-à-dire en-dessous de l'enceinte (2) avec son conduit (6) d'évacuation, et au-dessus du lit solide de la zone D.In FIG. 4, means (40) have been added, allowing the introduction of the light extraction phase L B above the bed of the dense phase D A , the light phase L B being injected against the current of the dense phase D A which flows from the separation zone A towards the enclosure (3). This injection allows the partial pressure of desorbed gases (hydrocarbons for example) rising from the extraction zone D to the enclosure (2) to decrease in the diluted solid phase (circulating from zone A towards the enclosure (3)). ) evacuation, and therefore promote desorption.
The means (40) are conventional means for introducing gas (such as a straight or circular pipe provided with orifices) which must respect a distribution of fluid as homogeneous as possible. These means (40) are therefore disposed at the level of zone C, that is to say below the enclosure (2) with its evacuation duct (6), and above the solid bed of zone D.
Sur la figure (5), on a schématisé un appareil selon la présente invention, et qui ne diffère de l'appareil décrit précédemment que par le fait que l'axe (X) du séparateur extracteur est positionné horizontalement, ce qui permet de diminuer la hauteur de l'équipement, et peut donc être avantageux dans certains cas. Il faut cependant maintenir l'axe de l'enceinte (3) vertical de façon à fluidiser correctement en phase dense.In Figure (5), there is shown schematically an apparatus according to the present invention, and which differs from the apparatus described above only in that the axis (X) of the extractor separator is positioned horizontally, which makes it possible to reduce the height of the equipment, and can therefore be advantageous in certain cases. However, the axis of the enclosure (3) must be kept vertical so as to fluidize correctly in the dense phase.
Afin d'améliorer le stripage dans l'enceinte (3) dans le lit fluidisé (9), des moyens visant à améliorer le contactage entre la phase légère L B et la phase dense D A peuvent être insérés dans le lit fluidisé (9). Ces moyens sont par exemple des tubes (107) disposés en rangées régulières sur la section de l'enceinte (3), et représentés sur la figure (5). On choisira par exemple de disposer des tubes de diamètre variant entre 0.02 et 0.08 m disposés à intervalle d'au moins une fois le diamètre des tubes. Ces tubes pourraient avantageusement être utilisés pour réchauffer le lit fluidisé et favoriser la désorption des produits de la réaction.In order to improve the stripping in the enclosure (3) in the fluidized bed (9), means aiming to improve the contacting between the light phase L B and the dense phase D A can be inserted in the fluidized bed (9) . These means are for example tubes (107) arranged in regular rows on the section of the enclosure (3), and shown in Figure (5). We will choose for example to have tubes of diameter varying between 0.02 and 0.08 m arranged at intervals of at least once the diameter of the tubes. These tubes could advantageously be used to heat the fluidized bed and promote the desorption of the reaction products.
Dans les séparateurs extracteurs selon l'invention le temps de séjour des solides constituants la phase dense D A dans le lit fluidisé (9) est habituellement d'environ 10 (s) secondes à environ 15 (min) minutes. Le plus souvent ce temps de séjour est d'environ 30 s à environ 10 min.In the extractor separators according to the invention, the residence time of the solids constituting the dense phase D A in the fluidized bed (9) is usually from about 10 (s) seconds to about 15 (min) minutes. Most often this residence time is from about 30 s to about 10 min.
Le plus souvent le rapport de la vitesse superficielle de la phase L B à la vitesse minimale de fluidisation (reliée aux propriétés de la phase dense D A et de la phase légère L B) est d'environ 1 : 1 à 500 : 1 et de préférence 10 : 1 à 100 : 1.Most often the ratio of the surface speed of phase L B to the minimum fluidization speed (related to the properties of dense phase D A and light phase L B ) is from about 1: 1 to 500: 1 and preferably 10: 1 to 100: 1.
Le temps de séjour des particules solides de la phase D A dans l'espace périphérique (11) (zones B et C) varie habituellement de 10-1 s à 100 s et préférentiellement par exemple dans un séparateur extracteur de diamètre D1 égal à 50 cm de 3 à 15 s.The residence time of the solid particles of phase D A in the peripheral space (11) (zones B and C) usually varies from 10 -1 s to 100 s and preferably for example in an extractor separator of diameter D 1 equal to 50 cm from 3 to 15 s.
Les séparateurs extracteurs selon l'invention peuvent être utilisés pour la séparation rapide, à partir d'un mélange M A, comprenant une phase dense D A et une phase légère L A, de ladite phase dense et de ladite phase légère et à l'extraction des produits adsorbés par ladite phase dense D A. Le mélange à séparer peut être un mélange obtenu à l'issue d'une réaction chimique et comprenant au moins une phase qui contribue à cette réaction.The extractor separators according to the invention can be used for the rapid separation, from a mixture M A , comprising a dense phase D A and a light phase L A , of said dense phase and of said light phase and extraction of the products adsorbed by said dense phase D A. The mixture to be separated can be a mixture obtained at the end of a chemical reaction and comprising at least one phase which contributes to this reaction.
Des essais ont été conduits sur un séparateur extracteur tel que celui représenté par la figure 3 ayant la géométrie suivante :
- enceinte (1) : cylindrique, de diamètre 5 cm, de longueur 75 cm munie d'une entrée tangentielle à section rectangulaire (2,5 cm x 1,3 cm, le plus grand côté étant parallèle à l'axe (X)) avec un toit hélicoïdal et un cône de stabilisation de 6 cm de hauteur.
- enceinte (2) : Ls = 12,5 cm, la sortie du conduit d'évacuation est située à 55 cm du niveau extrême de l'entrée tangentielle (la cote L2 est égale à 42,5 cm). Le diamètre externe de l'enceinte (2) est de 2,5 cm et son diamètre interne de 2,3 cm.
- enceinte (3) : cylindrique, de diamètre 30 cm, haute de 1,2 m.
- enclosure (1): cylindrical,
diameter 5 cm, length 75 cm provided with a tangential inlet with rectangular section (2.5 cm x 1.3 cm, the largest side being parallel to the axis (X)) with a helical roof and a 6 cm high stabilization cone. - enclosure (2): Ls = 12.5 cm, the outlet of the evacuation duct is located 55 cm from the extreme level of the tangential inlet (the dimension L 2 is equal to 42.5 cm). The external diameter of the enclosure (2) is 2.5 cm and its internal diameter of 2.3 cm.
- enclosure (3): cylindrical, 30 cm in diameter, 1.2 m high.
Le débit volumique Q2 de mélange MA gaz/catalyseur entrant est de 8,3 X 10-3 m3/s ce qui correspond à une vitesse superficielle de 25 m/s pour la phase légère présente dans le mélange MA à l'entrée du séparateur extracteur. Diverses expériences ont été conduites, le débit de la phase légère L B d'extradion (en volume Q1) ayant varié de 0 à 15 % du débit Q2. Dans ces conditions, la vitesse de passage dans l'espace périphérique (11) est inférieure à 20 cm/s.The volume flow rate Q 2 of mixture M A gas / incoming catalyst is 8.3 X 10 -3 m 3 / s which corresponds to a surface speed of 25 m / s for the light phase present in the mixture M A to l entry of the extractor separator. Various experiments were carried out, the flow rate of the light phase L B of extradion (in volume Q 1 ) having varied from 0 to 15% of the flow rate Q 2 . Under these conditions, the speed of passage through the peripheral space (11) is less than 20 cm / s.
Les résultats suivants ont été obtenus avec du catalyseur de FCC de diamètre moyen 65 micromètres dans les conditions ambiantes de température et pression. Les phases légères L A et L B étant de l'air.The following results were obtained with an FCC catalyst with an average diameter of 65 micrometers under ambient conditions of temperature and pressure. The light phases L A and L B being air.
Ils montrent qu'un tel séparateur extracteur est tout-à-fait opérationnel puisque dans le domaine de débit de phase L B, injecté à contre-courant (voir ratio Q1/Q2 correspondant à nos expériences) l'efficacité de séparation baisse relativement peu.
Pa = pression en amont de (4).
Pd = pression à la sortie du conduit (6) d'évacuation de la phase légère.
Pa = pressure upstream of (4).
Pd = pressure at the outlet of the light phase discharge conduit (6).
On voit donc que l'appareil qui fait l'objet de la présente invention présente des avantages majeurs sur les différents appareils qui sont proposés dans la littérature. Il permet d'effectuer une séparation rapide, une extraction en phase diluée et une extraction profonde en phase dense.It can therefore be seen that the device which is the subject of the present invention has major advantages over the various devices which are proposed in the literature. It allows rapid separation, diluted phase extraction and deep dense phase extraction.
Claims (20)
- Cocurrent cyclone separator extractor for the separation of a gas/solid mixture MA, having at least one dense phase DA and a light phase LA, into at least one dense phase and into at least one light phase, with the extraction of the gases sorbed by the solid, said separator extractor comprising:an enclosure (1), called the first external enclosure, which is elongated along an axis (X), which has a substantially circular cross-section, of internal diameter D1 and length L1, having at a first end, means for the introduction of the mixture MA by a so-called external inlet (4), said means making it possible to give at least to the light phase LA a helical movement in the flow direction of the mixture MA in said enclosure,a so-called internal enclosure (2), which is elongated along the axis (X), has a substantially circular cross-section of diameter D2, which is less than D1 and of length L2, which is less than L1, whose end close to the outer end (4) located at a distance LS less than L1 from the extreme level of the external inlet (4) constitutes the so-called internal inlet (5) by which penetrates at least part of the light phase LA, said enclosure being extended by at least one pipe (6) permitting the discharge of the light phase LA separated outside the first external enclosure,an enclosure (3), called the second external enclosure, having a substantially vertical axis of symmetry, connected to said first enclosure by an opening of diameter D1, said second enclosure collecting the separated dense phase DA having means (10) for the injection of a light extraction phase LB, injection taking place in countercurrent with respect to the flow of the separated dense phase and at least in part in said dense phase which is at least partly fluidized, and has at least one outlet (12) for the recovery of the at least partly desorbed dense phase DA.
- Separator extractor according to claim 1, wherein the external enclosure (3) is located in the extension of the first external enclosure along the axis (X).
- Separator extractor according to either of the preceding claims, wherein the second external enclosure (3) is elongated along an axis and has a substantially circular cross-section of diameter D greater than D1.
- Separator extractor according to any one of the preceding claims, wherein a vertical cylindrical well located on the axis of the second external enclosure (3) constitutes the dense phase outlet (12).
- Separator extractor according to any one of the preceding claims, wherein the dense phase passes out through a disengagement well.
- Separator extractor according to claim 5, wherein means for injecting the light fluidization phase are provided in the disengagement well.
- Separator extractor according to any one of the preceding claims, wherein the means (10) for the injection of the light extraction phase are constituted by a ring centered on the axis of the second enclosure (3) and provided with orifices directed towards the opening (7).
- Separator extractor according to any one of the preceding claims also having means (40) for light extraction phase injection above the dense phase bed and in countercurrent with respect to the separated dense phase flow.
- Separator extractor according to any one of the preceding claims comprising means (32) for rendering uniform the distribution of the separated dense phase arriving in the second external enclosure (3) and for breaking the flow on the wall of the solids.
- Separator extractor according to claim 9, wherein the means (32) are constituted by blades.
- Separator extractor according to claim 10, wherein the blades are fixed to the outer wall of the internal enclosure (2).
- Separator extractor according to any one of the preceding claims, wherein the pipe or pipes (6) are arranged in such a way that the light phase is discharged in a substantially axial direction with respect to the first external enclosure (1).
- Separator extractor according to any one of the claims 1 to 11, wherein the pipe or pipes (6) are arranged in such a way that the light phase is discharged in a direction substantially perpendicular to the axis of the first external enclosure (1).
- Separator extractor according to any one of the preceding claims, wherein the means for introducing the mixture MA are constituted by an inlet (4) tangential to the enclosure (1).
- Separator extractor according to any one of the preceding claims, wherein the means for introducing the mixture MA comprise blades (26) placed in the inlet (4).
- Separator extractor according to any one of the preceding claims, wherein the means for introducing the mixture MA comprise a helical roof.
- Separator extractor according to any one of the preceding claims, comprising a vortex stabilization cone (31) located at the inlet (4) along the axis facing the inlet (5).
- Separator extractor according to any one of the preceding claims, wherein the enclosure (3) has means for improving contacting between the light phase LB and the dense phase DA.
- Use of a separator extractor according to any one of the preceding claims for the rapid separation, from a mixture MA comprising the dense phase DA and a light phase LA, of said dense phase and said light phase and the extraction of the products adsorbed by said dense phase DA.
- Use according to claim 19, wherein the mixture to be separated is a mixture obtained at the end of a chemical reaction and having at least one phase contributing to said reaction.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9115063A FR2684566B1 (en) | 1991-12-05 | 1991-12-05 | CO-CURRENT CYCLONIC EXTRACTOR SEPARATOR. |
FR9115063 | 1991-12-05 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0545771A1 EP0545771A1 (en) | 1993-06-09 |
EP0545771B1 true EP0545771B1 (en) | 1996-09-18 |
Family
ID=9419696
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP92403149A Expired - Lifetime EP0545771B1 (en) | 1991-12-05 | 1992-11-23 | Concurrent cyclone extractor |
Country Status (9)
Country | Link |
---|---|
US (1) | US5586998A (en) |
EP (1) | EP0545771B1 (en) |
JP (1) | JP3275105B2 (en) |
AU (1) | AU657378B2 (en) |
CA (1) | CA2084633A1 (en) |
DE (1) | DE69213895T2 (en) |
ES (1) | ES2094322T3 (en) |
FR (1) | FR2684566B1 (en) |
ZA (1) | ZA929426B (en) |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2706136B1 (en) * | 1993-06-07 | 1995-07-28 | Inst Francais Du Petrole | Charge conversion device comprising a cyclonic co-current extractor separator. |
FR2780663B1 (en) * | 1998-07-02 | 2000-09-29 | Total Raffinage Distribution | METHOD OF EXTRACTIVE STRIPPING OF FLUIDIZED SOLID PARTICLES AND DEVICE FOR IMPLEMENTING SAME |
FR2798864B1 (en) * | 1999-09-24 | 2001-12-14 | Inst Francais Du Petrole | GAS / LIQUID SEPARATION SYSTEM FOR A HYDROCARBON CONVERSION PROCESS |
EP1379607B1 (en) * | 2001-04-20 | 2009-04-01 | Shell Internationale Researchmaatschappij B.V. | Fcc reactor vessel |
US7250140B2 (en) | 2002-04-11 | 2007-07-31 | Shell Oil Company | FCC reactor |
US7160518B2 (en) | 2002-04-11 | 2007-01-09 | Shell Oil Company | Cyclone separator |
JP4504256B2 (en) * | 2005-06-08 | 2010-07-14 | 武郎 吉田 | Cyclone separator |
JP2010511492A (en) * | 2006-11-30 | 2010-04-15 | ウエストレイク ロングビュー コーポレイション | High pressure separator |
RU2458297C1 (en) * | 2011-03-10 | 2012-08-10 | Общество С Ограниченной Ответственностью "Аэрогаз" | Gas mixture separation method |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4414100A (en) * | 1981-12-29 | 1983-11-08 | Chevron Research Company | Fluidized catalytic cracking |
US4455220A (en) * | 1982-12-23 | 1984-06-19 | Shell Oil Company | Separation of fluid cracking catalyst particles from gaseous hydrocarbons |
US4581205A (en) * | 1983-09-06 | 1986-04-08 | Mobil Oil Corporation | Closed cyclone FCC system with provisions for surge capacity |
CA1277276C (en) * | 1984-07-18 | 1990-12-04 | James H. Haddad | Fcc catalyst stripping method and apparatus |
US4731228A (en) * | 1986-06-16 | 1988-03-15 | Shell Oil Company | Reactor and horizontal cyclone separator with primary mass flow and secondary centrifugal separation of solid and fluid phases |
US5053082A (en) * | 1990-02-28 | 1991-10-01 | Conoco Inc. | Process and apparatus for cleaning particulate solids |
FR2662618B1 (en) * | 1990-06-05 | 1993-01-29 | Inst Francais Du Petrole | CO-CURRENT CYCLONIC SEPARATOR AND ITS APPLICATIONS. |
FR2662619B1 (en) * | 1990-06-05 | 1993-02-05 | Inst Francais Du Petrole | CO-CURRENT CYCLONIC MIXER-SEPARATOR AND ITS APPLICATIONS. |
FR2668720B1 (en) * | 1990-11-07 | 1993-06-11 | Stein Industrie | CYCLONE FOR SEPARATION BY CENTRIFUGATION OF A MIXTURE OF GASES AND SOLID PARTICLES WITH HEAT RECOVERY. |
FR2678280B1 (en) * | 1991-06-27 | 1993-10-15 | Institut Francais Petrole | METHOD AND DEVICE FOR CATALYTIC CRACKING OF A HYDROCARBON LOAD USING A CO-CURRENT CYCLONIC SEPARATOR. |
-
1991
- 1991-12-05 FR FR9115063A patent/FR2684566B1/en not_active Expired - Lifetime
-
1992
- 1992-11-23 ES ES92403149T patent/ES2094322T3/en not_active Expired - Lifetime
- 1992-11-23 DE DE69213895T patent/DE69213895T2/en not_active Expired - Fee Related
- 1992-11-23 EP EP92403149A patent/EP0545771B1/en not_active Expired - Lifetime
- 1992-12-03 AU AU29857/92A patent/AU657378B2/en not_active Ceased
- 1992-12-04 ZA ZA929426A patent/ZA929426B/en unknown
- 1992-12-04 JP JP32452592A patent/JP3275105B2/en not_active Expired - Fee Related
- 1992-12-04 CA CA002084633A patent/CA2084633A1/en not_active Abandoned
-
1995
- 1995-01-17 US US08/373,535 patent/US5586998A/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
EP0545771A1 (en) | 1993-06-09 |
DE69213895D1 (en) | 1996-10-24 |
ES2094322T3 (en) | 1997-01-16 |
AU657378B2 (en) | 1995-03-09 |
DE69213895T2 (en) | 1997-03-06 |
US5586998A (en) | 1996-12-24 |
FR2684566B1 (en) | 1994-02-25 |
FR2684566A1 (en) | 1993-06-11 |
CA2084633A1 (en) | 1993-06-06 |
AU2985792A (en) | 1993-06-10 |
JPH05269326A (en) | 1993-10-19 |
ZA929426B (en) | 1994-06-06 |
JP3275105B2 (en) | 2002-04-15 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP1017762B1 (en) | Separating and stripping device and its use in catalytic cracking on fluidised bed | |
CA2043947C (en) | Dual-flow cyclon separator and its uses | |
EP0545771B1 (en) | Concurrent cyclone extractor | |
EP0226483B1 (en) | Process and apparatus for the catalytic cracking of a hydrocarbon feedstock submitted to a pretreatment with solid particles having a poor activity | |
EP0852963B1 (en) | Separator for the direct centrifuge of the particles of a gaseous mixture and its use in a thermal cracker or FCC unit | |
EP1800728B1 (en) | New system for gas-solid separation and for stripping for fluidised bed catalytic cracking units | |
EP0502767B1 (en) | Process and apparatus for the catalytic conversion of an oxygenated compound into olefins | |
FR2827791A1 (en) | METHOD AND DEVICE FOR INTRODUCING A LIQUID-VAPOR MIXTURE INTO A RADIALLY SUPPLIED CYLINDRICAL DISTILLATION COLUMN | |
EP0573316B1 (en) | Process and apparatus for the catalytic cracking in two successive reaction zones | |
EP0291408B1 (en) | Steam cracking process in a fluidised-bed reaction zone | |
FR2767715A1 (en) | Separator and stripping device for removing particles from a gas flow | |
FR2706136A1 (en) | Device for converting a feedstock including a countercurrent cyclone extractor separator | |
EP0498726B1 (en) | Process and apparatus for the catalytic conversion of an oxygenated compound into olefins | |
WO2021115794A1 (en) | Device and method for gas-solid separation using catalytic cracking in a fluidized bed with an external wall for vertical pre-stripping | |
EP0536054B1 (en) | Improvements to devices for fluid catalytic cracking of hydrocarbon stocks | |
FR2678280A1 (en) | Process and device for the catalytic cracking of a hydrocarbon feedstock employing a concurrent cyclone separator | |
WO2021115893A1 (en) | Device and method for gas-solid separation using catalytic cracking in a fluidized bed with an under-window baffle | |
WO2021115892A1 (en) | Device and method for gas-solid separation using catalytic cracking in a fluidized bed with side openings | |
FR2781691A1 (en) | Device separating and stripping particles from a gas flow | |
BE541663A (en) | ||
BE712787A (en) | ||
FR2599376A1 (en) | Process and apparatus for catalytic cracking of a hydrocarbon feedstock subjected to a pretreatment using solid particles of low activity |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): BE DE ES GB IT NL |
|
17P | Request for examination filed |
Effective date: 19931119 |
|
17Q | First examination report despatched |
Effective date: 19951127 |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
ITF | It: translation for a ep patent filed |
Owner name: DE DOMINICIS & MAYER S.R.L. |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): BE DE ES GB IT NL |
|
REF | Corresponds to: |
Ref document number: 69213895 Country of ref document: DE Date of ref document: 19961024 |
|
GBT | Gb: translation of ep patent filed (gb section 77(6)(a)/1977) |
Effective date: 19961101 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2094322 Country of ref document: ES Kind code of ref document: T3 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed | ||
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GB Payment date: 20011022 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: BE Payment date: 20011127 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: NL Payment date: 20011130 Year of fee payment: 10 Ref country code: ES Payment date: 20011130 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20011211 Year of fee payment: 10 |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: IF02 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20021123 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20021124 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20021130 |
|
BERE | Be: lapsed |
Owner name: INSTITUT FRANCAIS DU *PETROLE Effective date: 20021130 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NL Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030601 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030603 |
|
GBPC | Gb: european patent ceased through non-payment of renewal fee | ||
NLV4 | Nl: lapsed or anulled due to non-payment of the annual fee |
Effective date: 20030601 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FD2A Effective date: 20031213 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED. Effective date: 20051123 |